CN107377968A - A kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation - Google Patents

A kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation Download PDF

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Publication number
CN107377968A
CN107377968A CN201710804617.2A CN201710804617A CN107377968A CN 107377968 A CN107377968 A CN 107377968A CN 201710804617 A CN201710804617 A CN 201710804617A CN 107377968 A CN107377968 A CN 107377968A
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CN
China
Prior art keywords
crucible
heater
composite powder
heterogeneous composite
injection
Prior art date
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Pending
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CN201710804617.2A
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Chinese (zh)
Inventor
吴朝阳
江志
樊希安
罗自贵
李光强
周乐君
许坤
郭雨怡
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
Anhui University of Technology AHUT
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Wuhan University of Science and Engineering WUSE
Anhui University of Technology AHUT
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Application filed by Wuhan University of Science and Engineering WUSE, Anhui University of Technology AHUT filed Critical Wuhan University of Science and Engineering WUSE
Priority to CN201710804617.2A priority Critical patent/CN107377968A/en
Publication of CN107377968A publication Critical patent/CN107377968A/en
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/16—Metallic particles coated with a non-metal
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/4417—Methods specially adapted for coating powder
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/442—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using fluidised bed process

Abstract

The invention discloses a kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation, belong to powder metallurgical technology.A kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the present invention, including body of heater, hollow pipe, crucible and spraying and blowing organ, wherein, heater is provided with body of heater, the hollow pipe passes through sidewall of the furnace body, its one end is connected by air inlet pipe with spraying and blowing organ, and its other end is connected with crucible bottom.The present invention has the characteristics of simple in construction, easy to use, efficiency high, and powder can be made, in fluidisation state, to avoid the generation of sintering curing phenomenon, prepared powder has the advantages that heterojunction structure disperse is uniform and performance difference is small in whole course of reaction.

Description

A kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation
Technical field
The invention belongs to powder metallurgical technology, the injection more particularly to a kind of heterojunction structure composite powder fluidizes system Standby device and preparation method.
Background technology
In powder metallurgical technology, existing research work shows that introducing heterojunction structure in dusty material can be effective The physicochemical characteristics such as improvement its stability, corrosion resistance and biocompatibility.And Heterogeneous Composite powder is every physical Energy index is with its preparation technology tight association, composition, purity, particle diameter and the microstructure of Heterogeneous Composite powder etc. to final products Performance play decisive role.By selecting different preparation methods and regulation related process parameters, can effectively control multiple Close phase composition and the microstructure of powder.So meet the dusty material of performance requirement to obtain, its technology of preparing is to closing weight Will.
At present, the conventional preparation method of related heterogeneous material compound has pack cementation method, sluny impregnation method, sol-gel Method, chemical vapour deposition technique and hot spray process etc., wherein, chemical vapour deposition technique has that even structure is controllable, technique weight Renaturation is good, can prepare thin structure, easily realizes the advantages that deposition different component material, is widely used to heterojunction structure composite Preparation.As Chinese patent CN 201110349812.3 discloses a kind of ZnO/SnO2The system of heterogeneous structural nano luminescent material Preparation Method, this application case use chemical vapour deposition technique, and Sn powder and Zn powder are placed in into aluminium oxide boat front end as source material, from Gold-plated silicon substrate is placed at a certain distance from source material, then aluminium oxide boat is placed in tube furnace, high temperature is carried out after vacuumizing and is added Heat, then be passed through oxygen and be incubated, gained white product is ZnO/SnO on substrate after cooling2Heterogeneous structural nano line lights Material.
And for example, it is different to disclose a kind of two-dimentional black phosphorus/Transition-metal dichalcogenide by Chinese patent CN 201610378900.9 Matter junction device and preparation method thereof, wherein, the two-dimentional Transition-metal dichalcogenide in this application case is using normal pressure chemical Prepared by vapour deposition process, its preparation technology parameter is as follows：Molybdenum, the dosage in tungsten source are 10-200mg, raw material MoO3、 WO3、MoS2、MoSe2、MoTe2、WS2、WSe2Or WTe2Solid；Sulphur, selenium, the dosage of tellurium source are 5-300mg, and raw material is sulphur powder, selenium Powder and tellurium powder；Growth pressure is 10-6-105Pa, argon flow amount 60-200sccm, hydrogen flowing quantity 5-100sccm, and growth is warm 600-1500 DEG C of degree, growth time 1-60min.
However, when preparing heterogeneous material compound using existing chemical vapour deposition technique, on the one hand, its preparation process is led to It is often to be carried out in transverse tube tube furnace or transverse tube chemical vapor deposition stove, it is different from block materials, due to the original accumulated in boiler tube Feed powder end meeting sintering curing under high temperature, and characteristic pockety, easily cause heterojunction structure and are unable to even dispersion, it is difficult to Meet to require the modified of material powder；On the other hand, because the material powder specific surface area of different-grain diameter is different, reacting Cheng Zhong, powder are different from the exposure level of reactant gas molecules so that the microcosmic knot of the same batch Heterogeneous Composite powder of preparation Larger difference between structure and performance be present, so as to reduce the quality of final products.
The content of the invention
1. invention technical problems to be solved
Existing chemical vapour deposition technique is used to prepare more than existing during heterogeneous material compound not it is contemplated that overcoming Foot, there is provided a kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation.Using the technology of the present invention Scheme can effectively avoid the generation of powder sintered solidification phenomenon, and preparing gained powder has the uniform performance of heterojunction structure disperse The features such as difference is small, suitable for the preparation of a variety of Heterogeneous Composite powder.
2. technical scheme
To reach above-mentioned purpose, technical scheme provided by the invention is：
A kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the present invention, including body of heater, hollow pipe, crucible And spraying and blowing organ, wherein, heater is provided with body of heater, the hollow pipe passes through sidewall of the furnace body, and its one end passes through air inlet pipe and spray Blow mechanism to be connected, its other end is connected with crucible bottom.
Further, described crucible includes sandwich construction, and high temperature resistant fluidized plate, resistance to height are provided between adjacent crucible layer Sieve aperture is machined with warm fluidized plate, and the screen-aperture on the high temperature resistant fluidized plate of upper strata is more than on lower floor's high temperature resistant fluidized plate Screen-aperture.
Further, described hollow pipe is provided with vibrating device.
Further, it is spiral shell between the crucible and high temperature resistant fluidized plate, and between crucible bottom and hollow pipe Line connects, and crucible overall processing is funnel-shaped structure.
Further, the hollow pipe is connected by flange with air inlet pipe, and the flange includes upper flange plate and lower flange Disk, wherein, upper flange plate is disc-shaped structure, and lower flange is circular ring, is provided between upper flange plate and lower flange First sealing ring, and upper flange plate is provided with injection air inlet, the injection air inlet is connected with air inlet pipe.
Further, hermatic door is provided with the top of the body of heater, the inwall of hermatic door is provided with the first high temperature resistance protective layer, institute State inboard wall of furnace body and be provided with the second high temperature resistance protective layer, and furnace body wall is provided with protection gas inflatable interface and suction interface；The sealing The 3rd sealing ring is provided between door and body of heater.
Further, vertically-mounted in the body of heater to have 6~8 heaters, the heater is centrosymmetric arrangement Body of heater and control power electric connection are passed in the surrounding of crucible, and at the top of heater.
Further, the side wall of the body of heater is also machined with data acquisition hole, and quartzy glass is embedded with data acquisition hole Glass, and data acquisition mechanism is provided with the outside of data acquisition hole, the receiving terminal of the data acquisition mechanism, data acquisition hole The central point of the axis of center line and crucible is located along the same line.
A kind of preparation method of Heterogeneous Composite powder based on injection fluidisation of the present invention, uses the said apparatus of the present invention Prepared by Heterogeneous Composite powder, Vibration on Start-up device, drive hollow pipe and crucible to be vibrated, so that the powder in crucible Powder stock is layered, and the powder stock of different-grain diameter is entered in different crucible layers by the sieve aperture on high temperature resistant fluidized plate, Inert gas and reacting gas are each led into from crucible bottom by spraying and blowing organ simultaneously, are in the powder stock in crucible Fluidized state.
Further, following steps are specifically included：
Step 1: powder stock loaded into crucible, open hermatic door, by silica crucible move in body of heater and by screw thread with Hollow pipe connects；The vibrating device on hollow pipe is opened, drives hollow pipe and crucible to be vibrated, so that the powder in crucible Raw material is layered, and closes hermatic door；
Step 2: starting vacuum extractor, the air in body of heater is evacuated to the vacuum of setting by suction interface, then lead to Overprotection gas inflatable interface is passed through inert gas；Open data acquisition mechanism and carry out data acquisition, then regulation blowing mechanism, lead to Cross air inlet pipe and be passed through same inert gas, make the powder stock in different crucible layers be in fluidizing state；
Step 3: opening control power supply, treat that heater is heated to the design temperature in body of heater, be incubated；
Step 4: regulation blowing mechanism, reacting gas is passed through by air inlet pipe, reacted the powder stock in crucible Prepare Heterogeneous Composite powder；
Step 5: reaction is completed, regulation blowing mechanism closes reacting gas, closing control power supply, stops heating, cooling.
3. beneficial effect
Using technical scheme provided by the invention, compared with prior art, there is following remarkable result：
(1) a kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the invention, its hollow pipe pass through body of heater Side wall, and one end of hollow pipe is connected by air inlet pipe with spraying and blowing organ, its other end is connected with crucible bottom, passes through injection Mechanism can be passed through inert gas from crucible bottom, with existing Heterogeneous Composite powder preparation transverse tube tube furnace or transverse tube chemistry gas Phase cvd furnace is compared, due to using fluidization technique is blown, making powder be blown and be in by inert gas in whole course of reaction Fluidize state, and hole produced between powder, so as to effectively avoid the sintering curing of material powder, while keep material powder with it is anti- Answer the abundant contact between gas molecule.
(2) preparation facilities of a kind of Heterogeneous Composite powder based on injection fluidisation of the invention, described crucible includes more Rotating fields, and the high temperature resistant fluidized plate comprising different pore size sieve aperture is provided between adjacent crucible layer, while coordinate with vibrating device Effect of vibration, so as to which so that the material powder in crucible is layered, the powder of different-grain diameter enters into different crucible layers Row reaction, that is, ensure each layer material powder and reactant gas molecules exposure level it is essentially identical, and then ensure same earthenware The structure of Heterogeneous Composite powder and performance difference are smaller obtained by being prepared in crucible layer, and uniformity is preferable.
(3) preparation facilities of a kind of Heterogeneous Composite powder based on injection fluidisation of the invention, the crucible and high temperature resistant It is to be threadedly coupled between fluidized plate, and between crucible bottom and hollow pipe, and crucible overall processing is funnel-shaped structure, is led to Cross and be threadedly coupled installation, dismounting consequently facilitating crucible, while the crucible to form the different numbers of plies can be assembled as needed.
(4) preparation method of a kind of Heterogeneous Composite powder based on injection fluidisation of the invention, is driven by vibrating device Hollow pipe and crucible are vibrated, so that the powder stock in crucible is layered, the powder stock of different-grain diameter passes through resistance to Sieve aperture on high temperature fluidized plate enters in different crucible layers, while each leads into indifferent gas from crucible bottom by spraying and blowing organ Body and reacting gas, the powder stock in crucible is set to be in fluidized state in whole course of reaction, so as to effectively anti- The only generation of sintering curing phenomenon, prepared powder have the characteristics of uniform performance difference of heterojunction structure disperse is small, are applicable In the preparation of a variety of Heterogeneous Composite powder, and its preparation facilities is simple in construction, easy to use, efficiency high.
(5) preparation method of a kind of Heterogeneous Composite powder based on injection fluidisation of the invention, using the gas of injection fluidisation Mutually deposition coating technology, it is simple to operate, not only in process of production without medium and purity is high, and because need not largely add high cost Material, such as high-purity gas and catalyst, reduce production cost and investment, have good industrial applications prospect.
Brief description of the drawings
Fig. 1 is the structural representation of the preparation facilities of the Heterogeneous Composite powder based on injection fluidisation of the present invention.
Label declaration in schematic diagram：
1st, hermatic door；2nd, the first high temperature resistance protective layer；3rd, the 3rd sealing ring；4th, heater；5th, body of heater；6th, the second high temperature resistant Protective layer；7th, quartz glass；8th, data acquisition mechanism；9th, crucible；10th, high temperature resistant fluidized plate；11st, hollow pipe；12nd, protection gas fills Gas interface；13rd, spraying and blowing organ；14th, it is blown air inlet pipe；15th, the first sealing ring；16th, adpting flange；17th, vibrating device；18th, Two sealing rings；19th, power supply is controlled；20th, suction interface.
Embodiment
To further appreciate that present disclosure, in conjunction with the drawings and specific embodiments, the present invention is described in detail.
Embodiment 1
As shown in figure 1, a kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the present embodiment, including body of heater 5th, hollow pipe 11, crucible 9 and spraying and blowing organ 13, wherein, heater 4 is provided with body of heater 5, the hollow pipe 11 passes through body of heater side Wall, its one end are connected by air inlet pipe 14 with spraying and blowing organ 13, and its other end is connected with the bottom of crucible 9.Pass through spraying and blowing organ 13 are passed through inert gas from the bottom of crucible 9 so that and powder is blown by inert gas in whole course of reaction and is in fluidisation state, And hole is produced between powder, so as to effectively avoid the sintering curing of material powder, while keep material powder and reacting gas Abundant contact between molecule, solve and Heterogeneous Composite powder is prepared using existing transverse tube tube furnace or transverse tube chemical vapor deposition stove It is insufficient existing for end.
Embodiment 2
As shown in figure 1, a kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the present embodiment, including body of heater 5th, hollow pipe 11, crucible 9 and spraying and blowing organ 13, wherein, heater 4 is provided with body of heater 5, the hollow pipe 11 passes through sidewall of the furnace body Injection hole, its one end is connected by air inlet pipe 14 with spraying and blowing organ 13, and its other end is connected with the bottom of crucible 9, the sky One end on heart pipe 11 close to spraying and blowing organ 13 is provided with vibrating device 17.The crucible 9 of the present embodiment includes sandwich construction, adjacent earthenware High temperature resistant fluidized plate 10 is provided between crucible layer, sieve aperture, and upper strata high temperature resistant fluidized plate 10 are machined with high temperature resistant fluidized plate 10 On screen-aperture be more than lower floor's high temperature resistant fluidized plate 10 on screen-aperture.Hollow pipe 11 and earthenware are driven by vibrating device 17 Crucible 9 vibrates, and so as to carry out vibrosieve to the powder stock in crucible 9, the powder of different-grain diameter enters different crucible layers Reacted, that is, ensure that each layer material powder and reactant gas molecules exposure level it is essentially identical, and then ensure same The gained structure of Heterogeneous Composite powder and the uniformity of performance are prepared in one crucible layer.
Embodiment 3
A kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the present embodiment, the substantially same embodiment of its structure 2, its difference essentially consists in：Between the crucible 9 and high temperature resistant fluidized plate 10 of the present embodiment, and the bottom of crucible 9 and hollow pipe 11 Between be threaded connection, and the overall processing of crucible 9 is funnel-shaped structure, consequently facilitating the installation and dismounting of crucible 9, and can be with According to the specific assembling number of plies for being actually needed selection crucible 9.
The hollow pipe 11 of the present embodiment uses stainless steel, and it is connected by flange 16 with air inlet pipe 14, the flange 16 include upper flange plate and lower flange, wherein, upper flange plate is disc-shaped structure and upper flange plate is provided with injection air inlet, Lower flange is circular ring and is fixedly connected with one end of stainless steel hollow pipe 11, is set between upper flange plate and lower flange There is the first sealing ring 15, and in the injection hole of the side wall of body of heater 5, i.e., second sealing ring is installed between sidewall of the furnace body and hollow pipe 11 18。
Embodiment 4
A kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation of the present embodiment, the substantially same embodiment of its structure 3, its difference essentially consists in：The top of body of heater 5 of the present embodiment is provided with hermatic door 1, and the inwall of hermatic door 1 is protected provided with the first high temperature resistant Sheath 2, the inwall of body of heater 5 is provided with the second high temperature resistance protective layer 6, and furnace body wall is provided with protection gas inflatable interface 12 and pumping connects Mouth 20；The 3rd sealing ring 3 is provided between the hermatic door 1 and body of heater 5.
Crucible 9 is vertically arranged to the inside center of body of heater 5 in the present embodiment, and vertically-mounted in body of heater 5 has 6~8 heatings Body 4, the heater 4, which is centrosymmetric, is arranged in the surrounding of crucible 9, and the top of heater 4 passes body of heater 5 and control power supply 19 electrical connections, the uniformity that may further ensure that powder heats in crucible 9 is set by the circular symmetric of heater 4.It is described The side wall of body of heater 5 is also machined with data acquisition hole, and quartz glass 7, and the outside in data acquisition hole are embedded with data acquisition hole Data acquisition mechanism 8, the axle of the receiving terminal of the data acquisition mechanism 8, the center line in data acquisition hole and crucible 9 are installed The central point of line is located along the same line.
Embodiment 5
A kind of preparation method of Heterogeneous Composite powder based on injection fluidisation of the present embodiment, its preparation facilities structure is the same as real Example 4 is applied, Vibration on Start-up device 17, drives hollow pipe 11 and crucible 9 to be vibrated, so that the powder stock in crucible 9 occurs Layering, the powder stock of different-grain diameter are entered in 9 layers different of crucibles by the sieve aperture on high temperature resistant fluidized plate 10, passed through simultaneously Spraying and blowing organ 13 each leads into inert gas and reacting gas from the bottom of crucible 9, makes the powder stock in crucible 9 be in fluidizing State, so as to effectively prevent the generation of sintering curing phenomenon, preparing gained powder has the uniform property of heterojunction structure disperse The characteristics of energy difference is small, suitable for the preparation of a variety of Heterogeneous Composite powder, and its preparation facilities is simple in construction, easy to use, effect Rate is high.The preparation method of the present embodiment, specifically includes following steps：
Step 1: powder stock is loaded into crucible 9, hermatic door 1 is opened, silica crucible 9 is moved in body of heater 5 and passes through spiral shell Line is connected with hollow pipe 11；The vibrating device 17 on hollow pipe 11 is opened, drives hollow pipe 11 and crucible 9 to be vibrated, so as to The powder stock in crucible 9 is layered, closes hermatic door 1；
Step 2: starting vacuum extractor, the air in body of heater 5 is evacuated to the vacuum of setting by suction interface 20, Again by protecting gas inflatable interface 12 to be passed through inert gas (argon gas or nitrogen can be used)；Open data acquisition mechanism 8 and enter line number According to collection, then regulation blowing mechanism 13, same inert gas is passed through by air inlet pipe 14, makes the powder in different crucible layers Raw material is in fluidizing state；
Step 3: opening control power supply 19, the design temperature that heater 4 is heated in body of heater 5 is treated, is incubated；
Step 4: regulation blowing mechanism 13, is passed through reacting gas by air inlet pipe 14, enters the powder stock in crucible 9 Row reaction prepares Heterogeneous Composite powder；
Step 5: reaction is completed, regulation blowing mechanism 13 closes reacting gas, closing control power supply 19, stops heating, drop Temperature.
The vapour deposition coating technology that the present embodiment is fluidized using injection, it is simple to operate, not only in process of production without Jie Matter and purity is high, and because without largely adding high cost material, such as high-purity gas and catalyst, reducing production cost and throwing Money, has good industrial applications prospect.
Schematically the present invention and embodiments thereof are described above, this describes no restricted, institute in accompanying drawing What is shown is also one of embodiments of the present invention, and actual structure is not limited thereto.So if common skill of this area Art personnel are enlightened by it, without departing from the spirit of the invention, without designing and the technical scheme for creativeness Similar frame mode and embodiment, protection scope of the present invention all should be belonged to.

Claims (10)

  1. A kind of 1. preparation facilities of the Heterogeneous Composite powder based on injection fluidisation, it is characterised in that：Including body of heater (5), hollow pipe (11), crucible (9) and spraying and blowing organ (13), wherein, heater (4) is provided with body of heater (5), the hollow pipe (11) passes through body of heater Side wall, its one end are connected by air inlet pipe (14) with spraying and blowing organ (13), and its other end is connected with crucible (9) bottom.
  2. A kind of 2. preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to claim 1, it is characterised in that： Described crucible (9) includes sandwich construction, and high temperature resistant fluidized plate (10), high temperature resistant fluidized plate (10) are provided between adjacent crucible layer On be machined with sieve aperture, and the screen-aperture on upper strata high temperature resistant fluidized plate (10) is more than on lower floor's high temperature resistant fluidized plate (10) Screen-aperture.
  3. A kind of 3. preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to claim 2, it is characterised in that： Described hollow pipe (11) is provided with vibrating device (17).
  4. 4. a kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to Claims 2 or 3, its feature exist In：It is screw thread between the crucible (9) and high temperature resistant fluidized plate (10), and between crucible (9) bottom and hollow pipe (11) Connection, and crucible (9) overall processing is funnel-shaped structure.
  5. 5. a kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to any one of claim 1-3, It is characterized in that：The hollow pipe (11) is connected by flange (16) with air inlet pipe (14), and the flange (16) includes upper flange plate And lower flange, wherein, upper flange plate is disc-shaped structure, and lower flange is circular ring, upper flange plate and lower flange Between be provided with the first sealing ring (15), and upper flange plate is provided with injection air inlet, the injection air inlet and air inlet pipe (14) phase Connection.
  6. 6. a kind of preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to any one of claim 1-3, It is characterized in that：Hermatic door (1) is provided with the top of the body of heater (5), the inwall of hermatic door (1) is provided with the first high temperature resistance protective layer (2), body of heater (5) inwall is provided with the second high temperature resistance protective layer (6), and furnace body wall is provided with protection gas inflatable interface (12) and taken out Gas interface (20)；The 3rd sealing ring (3) is provided between the hermatic door (1) and body of heater (5).
  7. A kind of 7. preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to claim 6, it is characterised in that： Vertically-mounted in the body of heater (5) to have 6~8 heaters (4), the heater (4), which is centrosymmetric, is arranged in crucible (9) Surrounding, and body of heater (5) is passed at the top of heater (4) and is electrically connected with control power supply (19).
  8. A kind of 8. preparation facilities of Heterogeneous Composite powder based on injection fluidisation according to claim 6, it is characterised in that： The side wall of the body of heater (5) is also machined with data acquisition hole, and quartz glass (7), and data acquisition are embedded with data acquisition hole Data acquisition mechanism (8), receiving terminal, the center line in data acquisition hole of the data acquisition mechanism (8) are installed on the outside of hole And the central point of the axis of crucible (9) is located along the same line.
  9. 9. a kind of preparation method of the Heterogeneous Composite powder based on injection fluidisation, it is characterised in that usage right requires to appoint in 1-8 Device described in one is prepared to Heterogeneous Composite powder, Vibration on Start-up device (17), drives hollow pipe (11) and crucible (9) Vibrated, so that the powder stock in crucible (9) is layered, the powder stock of different-grain diameter passes through high temperature resistant fluidized plate (10) sieve aperture on enters in different crucible (9) layers, while is each led into from crucible (9) bottom by spraying and blowing organ (13) lazy Property gas and reacting gas, make the powder stock in crucible (9) be in fluidized state.
  10. 10. a kind of preparation method of Heterogeneous Composite powder based on injection fluidisation according to claim 9, its feature exist In specifically including following steps：
    Step 1: powder stock is loaded into crucible (9), hermatic door (1) is opened, silica crucible (9) is moved in body of heater (5) and led to Screw thread is crossed to be connected with hollow pipe (11)；The vibrating device (17) on hollow pipe (11) is opened, drives hollow pipe (11) and crucible (9) Vibrated, so that the powder stock in crucible (9) is layered, close hermatic door (1)；
    Step 2: starting vacuum extractor, the air in body of heater (5) is evacuated to the vacuum of setting by suction interface (20), Again by protecting gas inflatable interface (12) to be passed through inert gas；Open data acquisition mechanism (8) and carry out data acquisition, then adjust Spraying and blowing organ (13), same inert gas is passed through by air inlet pipe (14), is in the powder stock in different crucible layers Fluidize state；
    Step 3: opening control power supply (19), the design temperature that heater (4) is heated in body of heater (5) is treated, is incubated；
    Step 4: regulation blowing mechanism (13), is passed through reacting gas by air inlet pipe (14), makes the powder stock in crucible (9) Carry out reaction and prepare Heterogeneous Composite powder；
    Step 5: reaction is completed, regulation blowing mechanism (13) closes reacting gas, closing control power supply (19), stops heating, drop Temperature.
CN201710804617.2A 2017-09-08 2017-09-08 A kind of preparation facilities and preparation method of the Heterogeneous Composite powder based on injection fluidisation Pending CN107377968A (en)

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